Manufacture of threads, ribbons, films, and the like from solutions of cellulose esters and cellulode ethers



Patented Oct. 13, 1931 UNITED ATE HENRI LOUISBARITHELEMY, or MILAZfi-ITALT, Assrenon 'ro RU'IHALDO co rAN me, or NEW xomzyimx f AeoRPonA'rIoN. or NEW YORK MANUFACTURE OF THREADS,

No Drawing. Application filed July 23, 1927, Serial No. 209,163, and in France'Deceinber 28, 19 26.

It consists in forcing a solutionobtainedin known manner (for inst-ance,' by dissolving cellulose, acetate, cellulose formats, cellulose nitrate or mixed esters) through a nozzle sprayed with or immersed in a special coagulating or precipitating liquid hereinafter d e. scribed; or more simply in distributing said solution in the form/of filaments orthin bands on means (such as a flat surface, an p I enables the filaments or films t0 be-cleaned endless band or a drum with a dull or polished surface) which is. sprayed with, or immersed in, said coagulating or precipitating liquid.v I I Said liquid may consist of an aqueous solution; of ammonium oleate, potassium oleate or sodium oleate, and these substances may be used either separately or mixed together; or it may consist, in general,lof anyaqueous solution which contains an ammonium or alkali salt of one or more'fatty acids (which may even'be sulfonated), for instance, am-

monium stearate, potassium palmitateor so-- dium recinoleate, sulfopalmitates 0r sulfon cinoleates of ammonium-or, sodiumletc. V

It has also been foundthat the addition of [members of a group 7 of compounds adapted to form aqueous 'emulsionsin the bath, still better results maybe obtained, for instance, in regard to the elasticity and lustre of the final product.

These compounds may be divided into four groups: Y j

(1) Simple alcohols and polyhidric alcohols; such as ordinary alcohol, butyl alcohol, glycol, glycerol, and. cyclohexanol, which may be employed separatelyor mixed together. r

(2) Hydrocarbons; such as'decane, tridecane, hexadecane,toluene, the three xylenes, tetralin, decalin, terpenes, sesquiterpenes, polyprenes, mineral oils and so on.

(3) Fatty acids of high molecular weight and their alkyl esters; such as mythyl oleate, 1

ethyl oleate, methyl stearate, and so on.

(4) The animal and vegetable oils which not only emulsify readily, but also with nIBBoNs; FILMS, AND THE'LIKE mom SOLUTIONS or CELLULOSE ns'rnns AND GELLULODE :srnnns I 4 o proper. concentration of the emulsifying agent, furnish what appear to the eye to be homogeneous mixtures with water.

It should be, noted that the invention differs substantlally from certain known proc:,

esses which aim at carrying out the spinning process in a single compound,for instance in oil of oils. o

The present invention presents a. great advantage over known processes, inasmuch as turpentine .or in animal or vegetable I When mineral or vegetable oils are added, the Y rior emulsification of the fatty substances in a very simple manner by merely washing in lukewarm water, as a result ofthe known cleansing action of alkaline soaps, the sulfo-L leatessulfopalmitates and the like.-

Furthermore, on coagulation, the threads are thoroughlylubricated by the coagulant vsolution itself, since the latter acts in the same manner as a true lubricating oil owing to .the simultaneous presence of a fatty oil wlth a sulforicmoleate or an alkaline soap.

This fact enables the filaments to besubjectedto mechanical treatment withffar great case than is possible in thecordinary spinning process for producingartificial silk; The presence of a soluble salt of a fatty acid or sulfofattyacid ofiers the'further advantage of considerably reducing surface tension, thereby on the one hand accelerating the diffusion of the solvent in the bath and on the other hand reducing the mutual adhesion of the Tfilaments in wthe productiono r artificial silk.

Instead of emulsifying agents specified ly they diminish the surface tension of the vwater. g v

The apparatus, in which-the precipitation is effected may be so designed that .thesolvent for the cellulose, esters can be continuously recovered by simple distillation, so that the drained and cooled bath may be used over and over again for precipitating fresh quantities of films or threads, on issuing from the dephlegmator.

Example 48 parts of a 50% solution of ammonium oleate are mixed with parts of neats-foot oil and 12 parts of mineral oil. A 19.8%. solution of cellulose acetate in acetone is threads, films, ribbons and the like, which consists in forcing a solution of cellulose acetate in acetone into an aqueous emulsion containing a solution of ammonium oleate mixed with neats-foot oil and mineral oil.

2. A process of manufacturing artificial threads, films, ribbons and the like, which consists in forcing an approximately 19.8% solution ofcellulose acetate in acetone into an aqueous emulsion containing about l-8-parts of a solution of ammonium oleate, 40 parts neats-foot oil and 12 parts of mineral oil. r

3. A process of. manufacturing artificial threads, films, ribbons-and thelike. which consists in introducing acetone solutions'of cellulose esters into an emulsified aqueous bath containing a slightly soluble organic liquid and an emulsifying agent.

A. A process of manufac'uring artificial threads, films, ribbons and the like, which consists in introducing a solution of cellulose acetate in acetone into aqueous bat-h comprising an oil emulsified in an aqueous solution of ammonium oleate.

5. A process of manufacturing artificial threads, films, ribbons and the like, which consists in introducing acetone solutions of cellulose esters into a mixture of an emulsifying agent in waterand an emulsified compound dispersed in the mixture.

6. A process of manufacturing artificial threads, films, ribbons and the like, which consists in precipitating or forcing acetone solutions of cellulose esters into an aqueous coagulating bath composed of an emulsifying agent in water and an emulsified compound dispersed in the mixture, said compound being a solvent of the solvent employed for the preparation of the cellulose acetate solution.

7. A process of manufacturing artificial threads, films, ribbons and the like, which consists in precipitating or forcing acetone solutions of cellulose esters into an emulsified mixture of water and compounds which are not solvents of esters of cellulose, and which compounds added to Water will diminish its surface tension.

8. A process of manufacturing artificial threads, films, ribbons and the like, which consists in precipitating or forcing acetone solutions of cellulose esters into an aqueous mixture containing oil and an emulsifying g t 9. A process of manufacturing artificial threads, films, ribbons and the like, which consists in coagulating cellulosic ester solutions in a mixture of water and a material giving an emulsion with water.

10. A process of manufacturing artificial threads, films, ribbons and the like, consisting in coagulating solutions of cellulose esters in an aqueous mixture composed of water, and an organic compound insoluble in water and a chemical compound which emulsifies the organic compound in the water.

11. A' process of manufacturing artificial threads, films, ribbons and the like, consisting in coagulating solutions of cellulose esters in a mixture of water, a material having the property of lowering the surface tension of water and of emulsifying fatty substances, and an organic solvent of the cellulose ester to be spun.

12. The manufacture of cellulosic products consisting in entering a solution of a cellulose ester in filament form into a coagulating bath consisting of an aqueous emulsion of oil. I

13. The manufacture of cellulosic products consisting in enteringa solution of a cellulose ester in filament form into Y a coagulating bath consisting of water and oil emulsified by means of a soap.

14. Aprocess of manufacturing artificial threads, films, ribbons and the like, which consists in precipitating an acetone solution ofa cellulose ester in an emulsified aqueous liquid mass containing acetone.

15. A process of manufacturing artificial threads films, ribbons and the like, which consists in, precipitating acetone solutions of cellulose esters in an emulsion of water and iquids which are not solvents of the cellulose ester used. p

In testimony whereof I afiix my signature.

HENRI LOUIS BARTHELEMY. 

